An experimental investigation of triboelectrification in cohesive and non-cohesive pharmaceutical powders

Abstract

A detailed experimental investigation has been undertaken of the triboelectrification process of the pharmaceutical excipient alpha-lactose monohydrate and selected drugs. Particle charge studies involved the design and construction of an apparatus to incorporate pneumatic powder feed, triboelectric charging via a cyclone separator and simultaneous powder charge (Q) and mass (M) measurements using a modified Faraday well. Preliminary studies showed the charging of the selected materials to be unaffected by relative humidity up to 84%, due to the very low hygroscopicity of the powders. Experiments using lactose size fractions with brass, steel and cellulose contact charging surfaces conducted at different feeder gas pressures, gave net electronegative specific charge values (Q/M) for the metal surfaces, and electropositive values for cellulose. Specific charge increased linearly with gas pressure for the metals, and non-linearly for cellulose. Samples of micronised lactose and beclomethasone dipropionate (BDP) showed more tendency than unmicronised samples to adhere to the contact surface which resulted in more complex charging processes. A novel system to analyse the charge and mass data in further detail was developed, giving relative Q/M values at unit time intervals. It is proposed that this will overcome the limitations of reliance on the final net specific charge value. Preliminary results indicated differences in the charging mechanism for lactose in contact with the two metal surfaces.     

Effects of Powder Velocity and Contact Materials on Tribocharging of Polymer Powders for Powder Coating Applications

Electrostatic powder deposition using corona charging is widely used in a plethora of industrial applications. Disadvantages of this technique are back corona onset and the Faraday penetration limitation. Another method to charge powders is to use tribochargers. Tribocharging depends upon the work function difference between the contacting materials and generates bipolarly charged particles. In this study, acrylic and epoxy powders were fluidized and charged by passing through stainless steel, copper, aluminum, and polycarbonate static mixers, respectively. The particle velocity and powder flow rate were varied to determine their effect on the net charge-to-mass ratio (Q/M) acquired by the powders. The Q/M increased rapidly with velocities between 1.5 to 2.5 m/s and stabilized for higher velocities but decreased with increasing powder flow rate at a constant velocity. The net positive or negative charge on each powder was determined to be dependant on the charger material. The use of an aluminum charger (net negative charge) in combination with a PTFE finger nozzle (net positive charge) resulted in a net powder Q/M of - 0.05 μC/g. The generation of an ion-free powder cloud with high bipolar charge but overall charge density of almost zero is anticipated to provide a better coverage of recessed areas.     

Portable Free-Fall Electrostatic Separator for Beneficiation of Charged Particulate Materials

A portable free-fall electrostatic separator capable of analyzing gram quantities of charged powders is presented. Unlike a Faraday pail, in which only the net average charge-to-mass (Q/M) ratio of the particles sampled by the instrument is measured, an electrostatic separator is capable of separately measuring the charge-to-mass ratios of positively and negatively charged sampled powders. Thus, with an electrostatic separator it is possible to measure the mass fractions of powders that are charged with different polarities and the respective charge-to-mass ratios, along with the mass fraction of particles that are uncharged or charged below a threshold level. We describe a method of measuring the total charge of the collected particles in real time by incorporating an electrometer to integrate the current flowing through the collecting electrode to the high voltage power supply. In this manner, both the total charge and total mass of powder deposited on the two electrodes are measured in near real time, providing information on charge-to-mass ratio of the aerosol cloud sampled. Such real time measurements are often needed to analyze the electrostatic charging properties of small quantities of dispersed powder, particularly in such applications where the charge characteristics are of high importance.     

TRIBOELECTRIC POWDER COATING: A PRACTICAL APPROACH FOR INDUSTRIAL USE

In the finishing industry the powder charge generated by friction in a tribo system is a useful alternative to the corona charging method. The charge by friction is called tribo-charge and is the result of frequent contacts of the powder particles with the interior insulating surfaces of the tribo gun. Different geometrical designs are incorporated for different systems e.g. through several holes or a ring slit.

Significant differences can be observed in the charging behaviour by either holes or slits which relate to the flow conditions. The dependence of the internal geometry and turbulent flow, particle velocity, powder mass flow rate and the volume of air flow influence the charging characteristics. An interesting new aspect is the growth of charge and the local distribution of charge during powder flow through a tribo gun. An examination has been made of the triboelectrical characteristics, the saturation charge and the charge/mass ratio.     

The Effect of Relative Humidity on Electrostatic Charge Decay of Drugs and Excipient Used in Dry Powder Inhaler Formulation

Electrostatic forces arising from charge accumulation on drug and excipient powders cause agglomeration and adhesion of particles to solid surfaces and problems during the manufacture and use of many pharmaceutical dosage forms, including dry powder inhalers (DPIs). The ability of materials to dissipate the acquired charge is therefore important and the aim of this work was to investigate the charge decay of salbutamol sulfate, ipratropium bromide monohydrate and α-lactose monohydrate. Differences in tri-phasic charge decay rates of the three materials in the order ipratropium bromide > lactose > salbutamol sulfate were demonstrated after corona charging and all materials showed an increased decay rate as the relative humidity was increased up to 86%. Preformulation knowledge of charge accumulation and decay in such materials will contribute to formulation, manufacture and performance of pharmaceutical dosage forms in general, and in particular DPIs.     

The effect of relative humidity on electrostatic charge decay of drugs and excipient used in dry powder inhaler formulation

Electrostatic forces arising from charge accumulation on drug and excipient powders cause agglomeration and adhesion of particles to solid surfaces and problems during the manufacture and use of many pharmaceutical dosage forms, including dry powder inhalers (DPIs). The ability of materials to dissipate the acquired charge is therefore important and the aim of this work was to investigate the charge decay of salbutamol sulfate, ipratropium bromide monohydrate and alpha-lactose monohydrate. Differences in tri-phasic charge decay rates of the three materials in the order ipratropium bromide > lactose > salbutamol sulfate were demonstrated after corona charging and all materials showed an increased decay rate as the relative humidity was increased up to 86%. Preformulation knowledge of charge accumulation and decay in such materials will contribute to formulation, manufacture and performance of pharmaceutical dosage forms in general, and in particular DPIs.     

Electrostatic Effects on Dispersion,Transport, and Deposition of Fine Pharmaceutical Powders: Development of an Experimental Method for Quantitative Analysis

Currently, there is no standard method for testing the electrostatic properties of pharmaceutical powders. The objective of this study was to develop a method of characterizing the dispersion, charging, and transport properties of fine powder flowing through tubes of different materials. Powders of known composition and size distribution were dispersed pneumatically and transported through a short section of tubing containing spiral baffle inserts of the same material to simulate powder flow in long sections of horizontal and vertical tubes with bends. The test powder was dispersed using ring jet suction and passed through the baffled tube to a sampling chamber, from which the powder cloud was sampled for particle size and electrostatic charge distribution measurement using an Electrical Single Particle Aerodynamic Relaxation Time (E-SPART) analyzer. Experimental data on the tribocharging and transport properties of different powders are presented along with an explanation of the charging mechanisms. Analyses of particle size and electrostatic charge distributions in real time and on a single particle basis using the E-SPART analyzer coupled with surface structure analyses with XPS and UPS showed that: (1) most powders are charged bipolarly with relatively high charge-to-mass ratio (Q/M) values that would have a strong effect on transport and deposition of powders; and (2) surface structures, particularly adsorbates, influence the work function and tribocharging of powder. Different methods, including plasma treatment, with minimal changes or contamination of the bulk properties of the powders are also suggested. pharmaceutical powders tribocharging dispersion work function charge distributions charge decay plasma treatment     

Electrostatic Effects on Dispersion, Transport, and Deposition of Fine Pharmaceutical Powders: Development of an Experimental Method for Quantitative Analysis

Currently, there is no standard method for testing the electrostatic properties of pharmaceutical powders. The objective of this study was to develop a method of characterizing the dispersion, charging, and transport properties of fine powder flowing through tubes of different materials. Powders of known composition and size distribution were dispersed pneumatically and transported through a short section of tubing containing spiral baffle inserts of the same material to simulate powder flow in long sections of horizontal and vertical tubes with bends. The test powder was dispersed using ring jet suction and passed through the baffled tube to a sampling chamber, from which the powder cloud was sampled for particle size and electrostatic charge distribution measurement using an Electrical Single Particle Aerodynamic Relaxation Time (E-SPART) analyzer. Experimental data on the tribocharging and transport properties of different powders are presented along with an explanation of the charging mechanisms. Analyses of particle size and electrostatic charge distributions in real time and on a single particle basis using the E-SPART analyzer coupled with surface structure analyses with XPS and UPS showed that: (1) most powders are charged bipolarly with relatively high charge-to-mass ratio (Q/M) values that would have a strong effect on transport and deposition of powders; and (2) surface structures, particularly adsorbates, influence the work function and tribocharging of powder. Different methods, including plasma treatment, with minimal changes or contamination of the bulk properties of the powders are also suggested.

pharmaceutical powders tribocharging dispersion work function charge distributions charge decay plasma treatment     

Interfacial Processes and Tribocharging: Effect of Plasma Surface Modification and Physisorption

The tribocharging characteristics of polymer powders have a significant impact on several industrial processes such as electrostatic powder coating and polymer powder processing. The nature of chemical species on the surface of powder influences the triboelectric charging characteristics. An atmospheric-pressure helium plasma was used to modify tribocharging properties of polystyrene microspheres and acrylic powders. Plasma surface modification reduced the magnitude of tribocharging for the test polymer powders. When tribocharged against stainless steel, the net charge-to-mass ratio (Q/M) for both polystyrene microspheres and acrylic powders was less than that for the control samples. Plasma surface modification also reduced the tribocharging of mannitol, a pharmaceutical powder, against stainless steel. Further, Mars simulant dust (JSC Mars 1) was used as a test sample to study the effect of carbon dioxide physisorption on tribocharging. The Q/M of the sample with physisorbed CO₂ was less than that of the control in all size ranges.     

Book Review

Triboelectrification affects particle adhesion and agglomeration and hence the formulation, manufacture, and use of dry powder inhaler (DPI) devices. Electrostatic charge measurement of two component mixes of spray-dried or crystalline lactose fine particles (<10 μm) 0, 5, 10, 15, 20, and 30% w/w with spray-dried or crystalline lactose 63–90 μm, respectively, has been undertaken using a system incorporating pneumatic transport of the mixed powders to a stainless steel cyclone charging device. The magnitude of charge on the mixes was shown to decrease with increased fine particle content, and there was no significant difference in charge for each concentration between spray-dried and crystalline lactose. Both the variation of charge and powder adhesion to the cyclone surface increased with increase in fine particle content. The proportion of fine particles in carrier systems in DPIs may thus have an important role where triboelectrification is involved.     

Modification of electrostatic charge on inhaled carrier lactose particles by addition of fine particles

Triboelectrification affects particle adhesion and agglomeration and hence the formulation, manufacture, and use of dry powder inhaler (DPI) devices. Electrostatic charge measurement of two component mixes of spray-dried or crystalline lactose fine particles (< 10 microns) 0, 5, 10, 15, 20, and 30% w/w with spray-dried or crystalline lactose 63-90 microns, respectively, has been undertaken using a system incorporating pneumatic transport of the mixed powders to a stainless steel cyclone charging device. The magnitude of charge on the mixes was shown to decrease with increased fine particle content, and there was no significant difference in charge for each concentration between spray-dried and crystalline lactose. Both the variation of charge and powder adhesion to the cyclone surface increased with increase in fine particle content. The proportion of fine particles in carrier systems in DPIs may thus have an important role where triboelectrification is involved.     

A tool for studying contact electrification in systems comprising metals and insulating polymers

We describe an analytical system for in situ measurement of the charge that develops by contact electrification when a ferromagnetic sphere rolls on the surface of a polymer. This system makes it possible to survey the ability of polymeric surfaces to charge by contact electrification. Because the measurement of charge using this tool does not require physical contact of the charged sphere with the measuring electrode, it also enables the kinetics of charging to be examined. The research has focused on the contact charging of spheres having a core-and-shell geometry (a common core of ferromagnetic steel, and a variable shell of thin films of metals, or metals with surface oxides) rolling on the surface of polymeric slabs; it has generated an internally consistent set of data that include the polarity and magnitude of charging for a homologous series of polymers that differ chemically in the pendant group on a polyethylene backbone.     

Evolution of potential distributions during the charging of nano-structured metal oxide films in air as response to sudden voltage application

Using metal oxide film structures, which were originally designed for gas sensing applications, we measured the charging and discharge currents and potential distributions on several metal oxide coatings after the application of an electrical potential against earth. The potential distributions show a specific charging of the surface with oxygen ions through the gas phase. The accumulated charge corresponds to that of the pseudocapacitors. Influence of air humidity has been found to be low, voltaic and temperature dependences of the charge are presented. The activation energy of discharge indicates a weak chemisorption of the charging oxygen species on the metal oxide surface.     

Compaction Properties of Spheronized Binary Granular Mixtures

Two spheronized granular formulations containing 20% anhydrous lactose/80% microcrystalline cellulose (MCC) and 80% anhydrous lactose/20% microcrystalline cellulose were blended in various proportions and compressed. Physical-mechanical properties of the resulting compacts were investigated using tableting indices and compared with powder mixtures of the same compositions. The compacts were compressed at a solid fraction of 0.80 for both powder and bead mixtures. An additional set of bead compacts were made at a solid fraction of 0.87. The thickness of the compacts was measured in the post-ejection stage to investigate their expansion behavior. The tensile strength with and without a stress concentrator and the dynamic indentation hardness of the compacts were determined. The brittle fracture index (BFI) and bonding index (BI) values were also calculated. The microstructure of the beads and compacts were investigated using scanning electron microscopy to observe the bonding phenomena. The results showed that the compacts made from beads underwent different compaction/consolidation behaviors than the powders of the same lactose/MCC compositions. For powdered compacts, the tensile strength with or without a stress concentrator increased with increasing MCC content while the compacts made from beads showed the opposite trend. However, this trend was not seen in the indentation hardness test. The resulting BFI values were all low due to the plastic nature of the materials selected. The BI values of the bead and powder compacts also exhibited opposite tendencies and reflected the divergent mechanical properties of the materials presented in granulated and powdered forms. Microstructure studies revealed the bonding states between the beads in the compacts. Discrepancies in mechanical properties were related to the compressibility, compactibility, and porosities of the excipients studied.     

Processing of nimesulide-PEG 400-PG-PVP solid dispersions: preparation,characterization, and in vitro dissolution

The objective of this investigation was to study the influence of dissolution enhancers such as polyethylene glycol 400, propylene glycol, polyvinylpyrrolidone K30, sodium lauryl sulfate, and Tween 80 on in vitro dissolution of a model active pharmaceutical material--nimesulide. Preliminary studies were conducted using a physical blend of nimesulide, and the adjuvants and solid dispersions were prepared using solvent evaporation and cogrinding methods. Aqueous solution of adjuvants was first triturated with nimesulide, followed by mixing with lactose and microcrystalline cellulose, and finally water was evaporated under vacuum in a cogrinding method. A 33 factorial design was adopted in a cogrinding method using the concentration of polyethylene glycol 400, propylene glycol, and polyvinylpyrrolidone K30 as independent variables. Tween 80 and sodium lauryl sulfate were added in all the batches. Full and reduced models were evolved for different dependent variables. The reduced models were validated using two checkpoints. Angle of repose < 35 degrees, percentage of drug released in 30 min (Q30) > 40%, 45 min (Q45) > 50%, and 120 min (Q12) > 60% were used as constraints for the selection of an optimized batch. Contour plots are presented for the selected dependent variables. Polyvinylpyrrolidone was found to be more effective in increasing the drug dissolution, compared with polyethylene glycol 400 and propylene glycol. The granule flow was adversely affected when high levels of liquid adjuvants were used in formulations. Wettability study was conducted to measure wetting time for pure drug and the optimized batch. Improved drug dissolution was attributed to improved wetting and the solubilizing effect of adjuvants from the pseudosolid dispersions of nimesulide. Significant improvement in drug dissolution was observed (Q120 = 70%), compared with pure drug powder (Q120 = 15%). In conclusion, dissolution of nimesulide can be modulated using an appropriate blend of pharmaceutical adjuvants.     

Control of particle charge by atmospheric pressure plasma jet (APPJ): A review

Atmospheric pressure plasma jets (APPJs) have more advantages regarding flexibility of operation than low pressure plasmas. Because the ions and/or electrons in the APPJ can be arbitrarily extracted to a gas-phase space by changing the DC bias voltage and efficiently deposited onto particle surfaces in an external electric field, this operating technique can be applied towards controlling particle charge. Several methods to control the particle charge using an APPJ system have already been reported. This article summarizes the specifications and operations of these systems, their mechanisms of charge transfer, and methods for particle charging, based on previously reported work. The methods are categorized into three groups, i.e., direct charging of particles, direct charging of a powder bed, and indirect charging of particles, and the corresponding experimental setups, procedures, results, and discussions are presented.     

某型延时起爆装置延期时间影响因素的研究

为实现某型延时起爆装置预定的延期时间，选用点火药硼/硝酸钾作为毫秒级延期药，通过对延期药原材料及装药结构的分析，尽可能地控制延期时间精度。主要针对延期药的原材料、装药密度、壳体材料、装药结构以及装药条件等对延期时间影响的机理及试验对比进行分析。经研究发现，延期药的延期时间和延期精度受诸多因素影响，一般来说药剂粒度适中且颗粒均匀，或提高装药压力，延期时间精度较高。其他因素（如装药壳体、装药结构、环境条件等）在不同程度上对延期时间精度也有影响，减少这些因素的影响对提高延期时间精度是十分必要的。     

Experimental study of triboelectric charging of polyethylene powders: Effect of humidity,impact velocity and temperature

The manufacturing and handling of polyethylene (PE) powders is associated with undesired charging, resulting in agglomeration of charged particles, wall sheeting and eventually leading to plugging of reactors/conveyors. In this work, we measured the triboelectric charging of PE powders using both sliding and shaking apparatuses in dependence on humidity, impact velocity of colliding particles and temperature of the colliding particles or of the wall. As expected, saturation charge of PE particles is reduced with increasing air humidity. However, in a more detailed study we observed that whenever we change the humidity, the saturation charge rapidly reaches the equilibrium value and no hysteresis in charging that might be caused, for example, by adsorption/desorption thermodynamics is observed. Saturation charge is believed to be independent of impact velocity; however, we show that the saturation charge is proportional to impact velocity in the system of PE particles of non-spherical shape. The charging is more pronounced as the temperature of PE particles increases, however, it is unchanged if only the metal wall in contact with the particles is heated. That is a different trend than observed for spherical metal particles (Greason, 2000).     

氧环境扫描电子显微分析:消除绝缘材料荷电效应的新方法

在环境扫描电镜(ESEM)中注入氧气,减少和消除绝缘样品表面在电子束辐照下产生的荷电效应.二次电子像的观察显示,在压力为130Pa～600Pa的ESEM中,氧气对Al2O3、Al(OH)3等氧化物、氢氧化物及生物样品的荷电补偿效果,优于常用的水蒸汽环境.通过吸收电流Ia的实时测试,评价了氧环境的荷电补偿效果.采用氧气减少表面荷电基于一个新的概念:在电子束的辐照下,电子受激解吸可造成表面氧亏损,使能带产生畸变,形成捕获电子的势阱.氧环境提供的氧离子可实现对氧空位的修复,从而消除了荷电效应.     

Deposition of functional cellulose films on titanium alloy surfaces

Titanium alloy (TiAl6V4) surfaces were treated with ultraviolet (UV) radiation to remove organic “contamination” molecules which remained on the surfaces after conventional cleaning processes. The UV-technique simultaneously revealed reactive surface hydroxyl groups at the metal surface which were monitored by the reaction with perfluorooctanoylchloride and application of Fourier-Transform infrared reflection-absorption spectroscopy and contact angle measurements, respectively. Two different cellulose polymers each made soluble in methanol by functionalized hydroxylalkyl-spacer groups and their mixtures were deposited on UV-treated TiAl6V4 surfaces. Atomic force microscopy measurements could reveal polymer films which covered the metal surfaces completely without defects. Differences were indicated in the surface structure, especially between the pure cellulose phosphate films and cinnamate containing cellulose films.